CN108383885A - From the technique and its purposes in anti-inflammatory for extracting Sophoricoside in the Fructus Sophorae - Google Patents
From the technique and its purposes in anti-inflammatory for extracting Sophoricoside in the Fructus Sophorae Download PDFInfo
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- CN108383885A CN108383885A CN201810408230.XA CN201810408230A CN108383885A CN 108383885 A CN108383885 A CN 108383885A CN 201810408230 A CN201810408230 A CN 201810408230A CN 108383885 A CN108383885 A CN 108383885A
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- fructus sophorae
- sophoricoside
- ethyl alcohol
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- 238000000034 method Methods 0.000 title claims abstract description 39
- ISQRJFLLIDGZEP-CMWLGVBASA-N Sophoricoside Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC=C(C=2C(C3=C(O)C=C(O)C=C3OC=2)=O)C=C1 ISQRJFLLIDGZEP-CMWLGVBASA-N 0.000 title claims abstract description 28
- ISQRJFLLIDGZEP-KJRRRBQDSA-N Sophoricoside Natural products O([C@@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@H](CO)O1)c1ccc(C=2C(=O)c3c(O)cc(O)cc3OC=2)cc1 ISQRJFLLIDGZEP-KJRRRBQDSA-N 0.000 title claims abstract description 28
- 230000003110 anti-inflammatory effect Effects 0.000 title claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 96
- 229930003944 flavone Natural products 0.000 claims abstract description 42
- 235000011949 flavones Nutrition 0.000 claims abstract description 42
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 claims abstract description 37
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 claims abstract description 37
- 150000002212 flavone derivatives Chemical class 0.000 claims abstract description 36
- 238000000605 extraction Methods 0.000 claims abstract description 25
- 230000005684 electric field Effects 0.000 claims abstract description 22
- 238000001704 evaporation Methods 0.000 claims abstract description 22
- 230000008020 evaporation Effects 0.000 claims abstract description 22
- 238000010828 elution Methods 0.000 claims abstract description 19
- 238000006911 enzymatic reaction Methods 0.000 claims abstract description 16
- 238000010008 shearing Methods 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000002425 crystallisation Methods 0.000 claims abstract description 7
- 230000008025 crystallization Effects 0.000 claims abstract description 7
- 238000010521 absorption reaction Methods 0.000 claims abstract description 6
- 235000019441 ethanol Nutrition 0.000 claims description 47
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 27
- 239000000843 powder Substances 0.000 claims description 20
- 238000012545 processing Methods 0.000 claims description 14
- 238000000874 microwave-assisted extraction Methods 0.000 claims description 11
- 108010059892 Cellulase Proteins 0.000 claims description 10
- 229940106157 cellulase Drugs 0.000 claims description 10
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 9
- 239000000287 crude extract Substances 0.000 claims description 8
- 239000003480 eluent Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000002250 absorbent Substances 0.000 claims description 7
- 230000002745 absorbent Effects 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 7
- 239000011347 resin Substances 0.000 claims description 7
- 229920005989 resin Polymers 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- 150000002213 flavones Chemical class 0.000 claims description 5
- 238000010025 steaming Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 15
- 239000013078 crystal Substances 0.000 description 12
- 235000021251 pulses Nutrition 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 7
- 238000005057 refrigeration Methods 0.000 description 7
- 238000001914 filtration Methods 0.000 description 6
- 229930003935 flavonoid Natural products 0.000 description 6
- 150000002215 flavonoids Chemical class 0.000 description 6
- 235000017173 flavonoids Nutrition 0.000 description 6
- 210000001367 artery Anatomy 0.000 description 5
- 210000002421 cell wall Anatomy 0.000 description 5
- 239000000284 extract Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
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- 108090000790 Enzymes Proteins 0.000 description 4
- 102000004190 Enzymes Human genes 0.000 description 4
- 229940088598 enzyme Drugs 0.000 description 4
- -1 flavone compound Chemical class 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 3
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 3
- REFJWTPEDVJJIY-UHFFFAOYSA-N Quercetin Chemical compound C=1C(O)=CC(O)=C(C(C=2O)=O)C=1OC=2C1=CC=C(O)C(O)=C1 REFJWTPEDVJJIY-UHFFFAOYSA-N 0.000 description 3
- 244000046101 Sophora japonica Species 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 229930182470 glycoside Natural products 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 description 3
- JMGZEFIQIZZSBH-UHFFFAOYSA-N Bioquercetin Natural products CC1OC(OCC(O)C2OC(OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5)C(O)C2O)C(O)C(O)C1O JMGZEFIQIZZSBH-UHFFFAOYSA-N 0.000 description 2
- 206010028980 Neoplasm Diseases 0.000 description 2
- ZVOLCUVKHLEPEV-UHFFFAOYSA-N Quercetagetin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=C(O)C(O)=C(O)C=C2O1 ZVOLCUVKHLEPEV-UHFFFAOYSA-N 0.000 description 2
- HWTZYBCRDDUBJY-UHFFFAOYSA-N Rhynchosin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=CC(O)=C(O)C=C2O1 HWTZYBCRDDUBJY-UHFFFAOYSA-N 0.000 description 2
- 235000010586 Sophora japonica Nutrition 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 201000011510 cancer Diseases 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- IVTMALDHFAHOGL-UHFFFAOYSA-N eriodictyol 7-O-rutinoside Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C=C3C(C(C(O)=C(O3)C=3C=C(O)C(O)=CC=3)=O)=C(O)C=2)O1 IVTMALDHFAHOGL-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- TZBJGXHYKVUXJN-UHFFFAOYSA-N genistein Natural products C1=CC(O)=CC=C1C1=COC2=CC(O)=CC(O)=C2C1=O TZBJGXHYKVUXJN-UHFFFAOYSA-N 0.000 description 2
- 235000006539 genistein Nutrition 0.000 description 2
- 229940045109 genistein Drugs 0.000 description 2
- IYRMWMYZSQPJKC-UHFFFAOYSA-N kaempferol Chemical compound C1=CC(O)=CC=C1C1=C(O)C(=O)C2=C(O)C=C(O)C=C2O1 IYRMWMYZSQPJKC-UHFFFAOYSA-N 0.000 description 2
- 210000004185 liver Anatomy 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 235000005875 quercetin Nutrition 0.000 description 2
- 229960001285 quercetin Drugs 0.000 description 2
- FDRQPMVGJOQVTL-UHFFFAOYSA-N quercetin rutinoside Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 FDRQPMVGJOQVTL-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- ALABRVAAKCSLSC-UHFFFAOYSA-N rutin Natural products CC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5 ALABRVAAKCSLSC-UHFFFAOYSA-N 0.000 description 2
- IKGXIBQEEMLURG-BKUODXTLSA-N rutin Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@@H]1OC[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-BKUODXTLSA-N 0.000 description 2
- 235000005493 rutin Nutrition 0.000 description 2
- 229960004555 rutoside Drugs 0.000 description 2
- UBSCDKPKWHYZNX-UHFFFAOYSA-N Demethoxycapillarisin Natural products C1=CC(O)=CC=C1OC1=CC(=O)C2=C(O)C=C(O)C=C2O1 UBSCDKPKWHYZNX-UHFFFAOYSA-N 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 208000032843 Hemorrhage Diseases 0.000 description 1
- GQODBWLKUWYOFX-UHFFFAOYSA-N Isorhamnetin Natural products C1=C(O)C(C)=CC(C2=C(C(=O)C3=C(O)C=C(O)C=C3O2)O)=C1 GQODBWLKUWYOFX-UHFFFAOYSA-N 0.000 description 1
- DCTLJGWMHPGCOS-UHFFFAOYSA-N Osajin Chemical compound C1=2C=CC(C)(C)OC=2C(CC=C(C)C)=C(O)C(C2=O)=C1OC=C2C1=CC=C(O)C=C1 DCTLJGWMHPGCOS-UHFFFAOYSA-N 0.000 description 1
- 208000001132 Osteoporosis Diseases 0.000 description 1
- OUZCFMSJGDEXRT-UHFFFAOYSA-N Scandinone Natural products O=C1C=2C(OC)=C(CC=C(C)C)C=3OC(C)(C)C=CC=3C=2OC=C1C1=CC=C(O)C=C1 OUZCFMSJGDEXRT-UHFFFAOYSA-N 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 208000002173 dizziness Diseases 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 210000003953 foreskin Anatomy 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- ZCOLJUOHXJRHDI-CMWLGVBASA-N genistein 7-O-beta-D-glucoside Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC(O)=C2C(=O)C(C=3C=CC(O)=CC=3)=COC2=C1 ZCOLJUOHXJRHDI-CMWLGVBASA-N 0.000 description 1
- 150000002338 glycosides Chemical class 0.000 description 1
- 238000003306 harvesting Methods 0.000 description 1
- 208000035861 hematochezia Diseases 0.000 description 1
- 208000014617 hemorrhoid Diseases 0.000 description 1
- 230000023597 hemostasis Effects 0.000 description 1
- 229940088597 hormone Drugs 0.000 description 1
- 239000005556 hormone Substances 0.000 description 1
- 210000000936 intestine Anatomy 0.000 description 1
- 230000003834 intracellular effect Effects 0.000 description 1
- CJWQYWQDLBZGPD-UHFFFAOYSA-N isoflavone Natural products C1=C(OC)C(OC)=CC(OC)=C1C1=COC2=C(C=CC(C)(C)O3)C3=C(OC)C=C2C1=O CJWQYWQDLBZGPD-UHFFFAOYSA-N 0.000 description 1
- 235000008696 isoflavones Nutrition 0.000 description 1
- 235000008800 isorhamnetin Nutrition 0.000 description 1
- IZQSVPBOUDKVDZ-UHFFFAOYSA-N isorhamnetin Chemical compound C1=C(O)C(OC)=CC(C2=C(C(=O)C3=C(O)C=C(O)C=C3O2)O)=C1 IZQSVPBOUDKVDZ-UHFFFAOYSA-N 0.000 description 1
- 235000008777 kaempferol Nutrition 0.000 description 1
- 210000002429 large intestine Anatomy 0.000 description 1
- 235000021374 legumes Nutrition 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- UXOUKMQIEVGVLY-UHFFFAOYSA-N morin Natural products OC1=CC(O)=CC(C2=C(C(=O)C3=C(O)C=C(O)C=C3O2)O)=C1 UXOUKMQIEVGVLY-UHFFFAOYSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 208000011580 syndromic disease Diseases 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- 150000003648 triterpenes Chemical class 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/26—Acyclic or carbocyclic radicals, substituted by hetero rings
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P29/00—Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Pain & Pain Management (AREA)
- Rheumatology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Medicinal Chemistry (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Pharmacology & Pharmacy (AREA)
- Animal Behavior & Ethology (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Saccharide Compounds (AREA)
Abstract
The invention belongs to technical field of plant extraction, the technique that Sophoricoside is extracted from the Fructus Sophorae is disclosed comprising following steps：Crushing → high pressure → electric field treatment → shearing → enzyme reaction → microwave alcohol extracting → evaporation → drying → absorption → elution → evaporation → drying → dissolving → crystallization.Present invention process is simple and feasible, and the recovery rate and purity of general flavone and Sophoricoside are high.
Description
Technical field
The invention belongs to technical field of plant extraction, and in particular to the technique of Sophoricoside be extracted from the Fructus Sophorae and its anti-inflammatory
Purposes in disease.
Background technology
The Fructus Sophorae is the fruit of legume Chinese scholartree Sophora japonica L., is the parts of generic medicinal plants that pharmacopeia is recorded, medicine
The ripe pod of winter harvesting should be usually used with the Fructus Sophorae.The drying Fructus Sophorae pod picked after Winter Solstice, it is cylinder, sometimes
It is bent, hangs between seed and shorten beaded into, be in brown or yellowish-brown after foreskin, seed is in brownish black；Theory of traditional Chinese medical science thinks,
The Fructus Sophorae is cold in nature, bitter, Return liver, large intestine channel, have clearing heat-fire, cooling blood and hemostasis function, have blood in stool suitable for intestines heat, hemorrhoid swell bleeding,
Liver thermal head pain, dizziness hot eyes.
Chemical research about the Fructus Sophorae had been reported that in the prior art, scientific research personnel's isolated number from the Fructus Sophorae
The ingredients such as kind flavonoids, alkaloids, triterpenes, amino acid and carbohydrate, wherein flavones ingredient content is higher, and is higher than other
The content of flavone compound in plant.In the Fructus Sophorae, the Flavonoids having determined at present include 20 kinds or more,
Total flavonoids substance mainly has Quercetin, Kaempferol, Isorhamnetin, genistein glycoside isoflavones, includes that a large amount of Chinese scholartree is more well
Sugar.There is good cancer-resisting and female hormone sample activity by the osajin of representative of genistein, to cancer, angiocarpy
Disease, osteoporosis and female climacteric syndrome have preventive and therapeutic effect.Rutin is the highest ingredient of content in Quercetin glycosides；Chinese scholartree
Angle glycosides is the main component of genistein glycosides.Currently, extraction Fructus Sophorae flavones technique have very much, mostly with use chemical reagent for
Master extracts, and there are the insecurity such as organic solvent residual for conventional extracting method, have potential threat to health,
The prior art improves extracting method, such as " process optimization of general flavone, food technology in the Enzymatic Extraction Fructus Sophorae
Science 2012 " extracts Fructus Sophorae flavones using enzyme process, has the advantages that nonhazardous, reaction condition is mild, but should
The defects of that there are enzyme dosages is larger for method, and recovery rate is relatively low, needs to be further improved it.Preamble work of the present invention is to total
Extracting flavonoids technique is improved, and has declared patented technology, and on this basis, inventor continues to have general flavone
Effect ingredient is detached.
Invention content
On the basis of applicant's achievement early period, the present invention continues to detach Fructus Sophorae general flavone cost-effectively, carries
It has supplied from the technique and its purposes in anti-inflammatory for extracting Sophoricoside in the Fructus Sophorae.
The present invention is achieved by the following technical solution：
The technique that Sophoricoside is extracted from the Fructus Sophorae comprising following steps：
Crushing → high pressure → electric field treatment → shearing → enzyme reaction → microwave alcohol extracting → evaporation → drying → absorption → elution → steaming
Hair → drying → dissolving → crystallization.
Specifically, the extraction process includes the following steps：
The Fructus Sophorae is taken, is crushed, 100-200 mesh sieve is crossed, obtains fructus sophorae powder, be subsequently placed in reactor, controlling pressure in reactor is
2-3MPa, pressurize 30-40s carry out impulse electric field processing；The water for adding 3-5 times of weight again, is sheared using high-speed shearing machine, so
Addition cellulase carries out enzyme reaction afterwards, then adds 70% ethyl alcohol of same volume, 60 DEG C is warming up to, using Microwave Extraction；It crosses
Extracting solution is collected in filter；Then into rotary evaporator, evaporation under reduced pressure removed ethyl alcohol, then vacuum freeze drying is obtained total
Flavones crude extract, then adsorbed with macroporous absorbent resin, with 70% ethanol elution, eluent is collected, rotation is re-introduced into and steams
It sends out in device, extractive of general flavone is made in evaporation under reduced pressure removed ethyl alcohol, last vacuum freeze drying；It is added into extractive of general flavone
The ethyl acetate of five times of weight, stirs evenly, and then filters, and collects insoluble matter, then 85% ethyl alcohol is added dropwise into insoluble matter, side drop
Edged heats, while being stirred with 100rpm, until insoluble matter is completely dissolved, is subsequently placed in 30min under 0 DEG C of environment, filters, and collects knot
Brilliant object to get.
Preferably, the field strength 10kv/cm of the impulse electric field, total processing time are 200 μ s, and pulse width is 4 μ s, pulse
Frequency is 400pps.
Preferably,
The shear time 3min of the high-speed shearing machine, shear velocity 5000rpm.
Preferably,
The enzyme reaction condition is：According to 10,000-2 ten thousand U:The ratio of 100g fructus sophorae powders adds cellulase, controls enzyme reaction temperature
It is 35 DEG C, reaction time 60-90min.
Preferably,
The condition of the Microwave Extraction is power 400-600W, extraction time 30-50min.
Sophoricoside prepared by the extraction process is also claimed in the present invention.
Purposes of the Sophoricoside of the present invention in anti-inflammatory.
It includes but is not limited to mainly the following aspects that the technology of the present invention, which uses above-mentioned technique, advantage,：
Fructus Sophorae close structure due to cell wall is rich in cellulose and hemicellulose, directly ultrasound or Microwave Extraction be difficult to make effectively at
Divide and be fully dissolved out, the present invention makes cell wall be pressurized and deformation or even partial rupture using HIGH PRESSURE TREATMENT first, then carries out arteries and veins
Electric field treatment is rushed, enzymolysis processing can be carried out to the cellulose of cell wall using cellulase to cell wall into eleven punch 11, on
It states method and multiple-disruption has been carried out to cell wall by synergistic effect, intracellular organic matter dissolution rate is high, and extraction advantage is more obvious, and
And it is simple for process feasible, extraction time is shortened, recovery rate and purity also accordingly improve；
There are the insecurity such as organic solvent residual for conventional extracting method, have potential threat to health.The present invention subtracts
It is few to use chemical organic formulations, improve the security performance of extract；
The present invention uses kinds of processes technology, by high pressure, impulse electric field, the shearing of high speed machine power, enzyme process and microwave alcohol extracting method
Be combined together, method is combined, realize have complementary advantages, make up the disadvantage of single technique, have low energy consumption, efficiency
Height, the features such as not destroying active ingredient, to can get higher extraction efficiency and purity；
The present invention dissolves other types of soluble flavone substance using ethyl acetate, then utilizes Sophoricoside in cold and hot ethyl alcohol
Different solubility, Fructus Sophorae glycosidal crystalline is precipitated, yield and purity are high, can be applied to the drug of anti-inflammatory.
Description of the drawings
Fig. 1：The influence of microwave power and time to general flavone yield.
Specific implementation mode
Those skilled in the art can use for reference present disclosure, be suitably modified technological parameter realization.In particular, it should be pointed out that
All similar substitutions and modifications are apparent to those skilled in the art, they are considered as being included in this hair
It is bright.The product and method of the present invention is described by preferred embodiment, and related personnel can obviously not depart from this hair
Product as described herein and method are modified or are suitably changed and combined in bright content, spirit and scope, to realize and answer
Use the technology of the present invention.For a further understanding of the present invention, the following describes the present invention in detail with reference to examples.
Embodiment 1
The technique that Sophoricoside is extracted from the Fructus Sophorae comprising following steps：
Crushing → high pressure → electric field treatment → shearing → enzyme reaction → microwave alcohol extracting → evaporation → drying → absorption → elution → steaming
Hair → drying → dissolving → crystallization.
It specifically includes：
The Fructus Sophorae is taken, is crushed, is sieved with 100 mesh sieve, obtain fructus sophorae powder, be subsequently placed in reactor, it is 3MPa to control pressure in reactor,
Pressurize 30s carries out impulse electric field processing, the field strength 10kv/cm of electric field, and total processing time is 200 μ s, and pulse width is 4 μ s, arteries and veins
It is 400pps to rush frequency；Then the water for adding 5 times of weight shears 3min, shear velocity 5000rpm using high-speed shearing machine,
According still further to 20,000 U:The ratio of 100g fructus sophorae powders adds cellulase, and control enzyme reaction temperature is 35 DEG C, reaction time 60min,
Then 70% ethyl alcohol for adding same volume, is warming up to 60 DEG C, and using Microwave Extraction, control microwave power is 600W, extraction time
For 30min；Extracting solution is collected in filtering；Then into rotary evaporator, evaporation under reduced pressure removed ethyl alcohol, then vacuum refrigeration
Dry obtained general flavone crude extract, then adsorbed with AB-8 type macroporous absorbent resins, with 70% ethanol elution of 2BV, elution speed
Degree is 0.5BV/h, collects eluent, is re-introduced into rotary evaporator, evaporation under reduced pressure removed ethyl alcohol, and last vacuum refrigeration is dry
Dry obtained extractive of general flavone；The ethyl acetate that five times of weight is added into extractive of general flavone, stirs evenly, then filters,
Insoluble matter is collected, then 85% ethyl alcohol is added dropwise into insoluble matter, is heated when being added dropwise, while being stirred with 100rpm, until insoluble matter is complete
Dissolving, be subsequently placed in 30min under 0 DEG C of environment, filter, collect crystal to get.Crystal is used into highly effective liquid phase chromatographic system
Detection（Operating process can refer to " HPLC while measuring the rutin in the Fructus Sophorae and Sophoricoside ", West China drug magazine 2010）, claim
The weight for recrystallizing object, analyzes the content and purity of Sophoricoside, wherein being calculated with fructus sophorae powder 1000g, Sophoricoside in fructus sophorae powder
Content is 4.71%, and collection crystal is 45.8g, and the purity of Sophoricoside is 95.1% in crystal, and the yield of Sophoricoside is
92.5%。
Embodiment 2
The technique that Sophoricoside is extracted from the Fructus Sophorae comprising following steps：
Crushing → high pressure → electric field treatment → shearing → enzyme reaction → microwave alcohol extracting → evaporation → drying → absorption → elution → steaming
Hair → drying → dissolving → crystallization.
It specifically includes：
The Fructus Sophorae is taken, is crushed, 200 mesh sieve is crossed, obtains fructus sophorae powder, be subsequently placed in reactor, it is 2MPa to control pressure in reactor,
Pressurize 40s carries out impulse electric field processing, the field strength 10kv/cm of electric field, and total processing time is 200 μ s, and pulse width is 4 μ s, arteries and veins
It is 400pps to rush frequency；Then the water for adding 4 times of weight shears 3min, shear velocity 5000rpm using high-speed shearing machine,
According still further to 10,000 U:The ratio of 100g fructus sophorae powders adds cellulase, and control enzyme reaction temperature is 35 DEG C, reaction time 90min,
Then 70% ethyl alcohol for adding same volume, is warming up to 60 DEG C, and using Microwave Extraction, control microwave power is 500W, extraction time
For 60min；Extracting solution is collected in filtering；Then into rotary evaporator, evaporation under reduced pressure removed ethyl alcohol, then vacuum refrigeration
Dry obtained general flavone crude extract, then adsorbed with HPD450 type macroporous absorbent resins, with 70% ethanol elution of 3BV, elution
Speed is 1BV/h, collects eluent, is re-introduced into rotary evaporator, evaporation under reduced pressure removed ethyl alcohol, and last vacuum refrigeration is dry
Dry obtained extractive of general flavone；The ethyl acetate that five times of weight is added into extractive of general flavone, stirs evenly, then filters,
Insoluble matter is collected, then 85% ethyl alcohol is added dropwise into insoluble matter, is heated when being added dropwise, while being stirred with 100rpm, until insoluble matter is complete
Dissolving, be subsequently placed in 30min under 0 DEG C of environment, filter, collect crystal to get.After testing, in crystal Sophoricoside purity
It is 94.7%, the yield of Sophoricoside is 93.1%.
Comparative example 1
The technique that Sophoricoside is extracted from the Fructus Sophorae comprising following steps：
The Fructus Sophorae is taken, is crushed, is sieved with 100 mesh sieve, obtain fructus sophorae powder, be subsequently placed in reactor, impulse electric field processing is carried out, electric field
Field strength 10kv/cm, total processing time are 200 μ s, and pulse width is 4 μ s, pulse frequency 400pps；Then 5 times of weight are added
Water, using high-speed shearing machine shear 3min, shear velocity 5000rpm, according still further to 20,000 U:The ratio of 100g fructus sophorae powders is added
Cellulase, control enzyme reaction temperature are 35 DEG C, reaction time 60min, then add 70% ethyl alcohol of same volume, heating
To 60 DEG C, using Microwave Extraction, control microwave power is 500W, extraction time 60min；Extracting solution is collected in filtering；Then into
Enter into rotary evaporator, evaporation under reduced pressure removed ethyl alcohol, then vacuum freeze drying is made general flavone crude extract, then with AB-8 types
Macroporous absorbent resin is adsorbed, and with 70% ethanol elution of 2BV, elution speed 0.5BV/h collects eluent, is again introduced into
Into rotary evaporator, extractive of general flavone is made in evaporation under reduced pressure removed ethyl alcohol, last vacuum freeze drying；It is extracted toward general flavone
The ethyl acetate that five times of weight is added in object, stirs evenly, then filters, and collects insoluble matter, then 85% second is added dropwise into insoluble matter
Alcohol is heated when being added dropwise, while being stirred with 100rpm, until insoluble matter is completely dissolved, is subsequently placed in 30min under 0 DEG C of environment, mistake
Filter, collect crystal to get.
Comparative example 2
The technique that Sophoricoside is extracted from the Fructus Sophorae comprising following steps：
The Fructus Sophorae is taken, is crushed, is sieved with 100 mesh sieve, obtain fructus sophorae powder, be subsequently placed in reactor, it is 3MPa to control pressure in reactor,
Then pressurize 30s adds the water of 5 times of weight, 3min, shear velocity 5000rpm, according still further to 2 are sheared using high-speed shearing machine
Ten thousand U:The ratio of 100g fructus sophorae powders adds cellulase, and control enzyme reaction temperature is 35 DEG C, then reaction time 60min adds
70% ethyl alcohol for adding same volume, is warming up to 60 DEG C, and using Microwave Extraction, control microwave power is 400W, and extraction time is
60min；Extracting solution is collected in filtering；Then into rotary evaporator, evaporation under reduced pressure removed ethyl alcohol, then vacuum refrigeration is dry
Dry obtained general flavone crude extract, then adsorbed with AB-8 type macroporous absorbent resins, with 70% ethanol elution of 2BV, elution speed
For 0.5BV/h, eluent is collected, is re-introduced into rotary evaporator, evaporation under reduced pressure removed ethyl alcohol, last vacuum freeze drying
Extractive of general flavone is made；The ethyl acetate that five times of weight is added into extractive of general flavone, stirs evenly, then filters, and receives
Collect insoluble matter, then 85% ethyl alcohol is added dropwise into insoluble matter, is heated when being added dropwise, while being stirred with 100rpm, until insoluble matter is completely molten
Solution, be subsequently placed in 30min under 0 DEG C of environment, filter, collect crystal to get.
Comparative example 3
The technique that Sophoricoside is extracted from the Fructus Sophorae comprising following steps：
The Fructus Sophorae is taken, is crushed, is sieved with 100 mesh sieve, obtain fructus sophorae powder, be subsequently placed in reactor, it is 3MPa to control pressure in reactor,
Pressurize 30s carries out impulse electric field processing, the field strength 10kv/cm of electric field, and total processing time is 200 μ s, and pulse width is 4 μ s, arteries and veins
It is 400pps to rush frequency；Then the water for adding 5 times of weight shears 3min, shear velocity 5000rpm using high-speed shearing machine,
Then 70% ethyl alcohol for adding same volume, is warming up to 60 DEG C, and using Microwave Extraction, control microwave power is 500W, extraction time
For 50min；Extracting solution is collected in filtering；Then into rotary evaporator, evaporation under reduced pressure removed ethyl alcohol, then vacuum refrigeration
Dry obtained general flavone crude extract, then adsorbed with AB-8 type macroporous absorbent resins, with 70% ethanol elution of 2BV, elution speed
Degree is 0.5BV/h, collects eluent, is re-introduced into rotary evaporator, evaporation under reduced pressure removed ethyl alcohol, and last vacuum refrigeration is dry
Dry obtained extractive of general flavone；The ethyl acetate that five times of weight is added into extractive of general flavone, stirs evenly, then filters,
Insoluble matter is collected, then 85% ethyl alcohol is added dropwise into insoluble matter, is heated when being added dropwise, while being stirred with 100rpm, until insoluble matter is complete
Dissolving, be subsequently placed in 30min under 0 DEG C of environment, filter, collect crystal to get.
Comparative example 4
The technique that Sophoricoside is extracted from the Fructus Sophorae comprising following steps：
The Fructus Sophorae is taken, is crushed, is sieved with 100 mesh sieve, obtain fructus sophorae powder, be subsequently placed in reactor, it is 3MPa to control pressure in reactor,
Pressurize 30s carries out impulse electric field processing, the field strength 10kv/cm of electric field, and total processing time is 200 μ s, and pulse width is 4 μ s, arteries and veins
It is 400pps to rush frequency；Then the water for adding 5 times of weight, according still further to 20,000 U:The ratio of 100g fructus sophorae powders adds cellulase, control
Enzyme reaction temperature processed is 35 DEG C, reaction time 60min, then adds 70% ethyl alcohol of same volume, is warming up to 60 DEG C, is used
Microwave Extraction, control microwave power are 500W, extraction time 60min；Extracting solution is collected in filtering；It is steamed then into rotation
It sends out in device, evaporation under reduced pressure removed ethyl alcohol, then vacuum freeze drying is made general flavone crude extract, then with AB-8 type macroporous absorption trees
Fat is adsorbed, and with 70% ethanol elution of 2BV, elution speed 0.5BV/h collects eluent, is re-introduced into rotary evaporation
In device, extractive of general flavone is made in evaporation under reduced pressure removed ethyl alcohol, last vacuum freeze drying；Five are added into extractive of general flavone
The ethyl acetate of times weight, stirs evenly, then filters, and collects insoluble matter, then 85% ethyl alcohol is added dropwise into insoluble matter, and side is added dropwise
Side is heated, while being stirred with 100rpm, until insoluble matter is completely dissolved, is subsequently placed in 30min under 0 DEG C of environment, is filtered, and crystallization is collected
Object to get.
Embodiment 3
Determination of Total Flavonoids：By taking the Fructus Sophorae of southern shandong area as an example, present invention experiment uses the 1000g Fructuss Sophorae, HPLC methods to measure fructus sophorae powder
The content of middle general flavone is 19.7%, experiment group difference selection example 1 and comparative example 1-4.Show that general flavone carries by weighing
The weight of object, HPLC methods is taken to measure general flavone content in extract, calculate the yield of general flavone, calculation formula：Yield=（It (carries
Take quality × content of object)/（Fructus Sophorae quality × content））× 100%.Concrete outcome is shown in Table 1：
Table 1
| Group | Fructus sophorae powder weight（g） | Extractive of general flavone（g） | General flavone content % in extract | Yield % |
| Embodiment 1 | 1000 | 245.9 | 75.8 | 94.6 |
| Comparative example 1 | 1000 | 234.7 | 70.4 | 83.9 |
| Comparative example 2 | 1000 | 221.8 | 68.1 | 76.7 |
| Comparative example 3 | 1000 | 218.3 | 62.6 | 69.4 |
| Comparative example 4 | 1000 | 247.6 | 72.9 | 91.6 |
The present invention also has detected the weight of embodiment 1 and the crystal of comparative example 1-4 and the content of Sophoricoside in crystal, tool
Body is shown in Table 2：
Table 2
| Group | Fructus sophorae powder weight（g） | Crystal weight（g） | Content % |
| Embodiment 1 | 1000 | 45.8 | 92.5 |
| Comparative example 1 | 1000 | 41.6 | 91.4 |
| Comparative example 2 | 1000 | 42.9 | 90.6 |
| Comparative example 3 | 1000 | 38.7 | 91.7 |
| Comparative example 4 | 1000 | 44.8 | 92.1 |
As shown in upper table 1-2, general flavone yield and purity are above comparative example 1-4 in 1 group of embodiment, are crystallized in 1 group of embodiment
The weight and Sophoricoside content of object reach highest in each group；The present invention uses kinds of processes technology, by high pressure, pulse
Electric field, the shearing of high speed machine power, enzyme process and microwave alcohol extracting method are combined together, and method is combined, and realize that advantage is mutual
It mends, makes up the disadvantage of single technique, have that low energy consumption, it is efficient, the features such as not destroying active ingredient, higher to can get
Extraction efficiency and purity.
Embodiment 4
The influence of microwave power and time to yield, setting microwave power is respectively 200w, 400w, 600w, 800w, 1000w, micro-
The wave time is respectively 10,20,30,40,50,60,70,80min.As shown in Figure 1, microwave power increases or microwave treatment time increases
The yield of general flavone can be improved by adding, but when microwave power increases to after 600w, yield is not further added by, and is reduced instead,
It may be that power is too big, Flavonoid substances caused to be destroyed；The microwave time within 50min, yield promoted it is apparent, with when
Between increase, there is no significant changes for yield.Therefore, the present invention selects microwave power in 400-600w, and the microwave time is 30-
50min。
Finally, it should also be noted that it is listed above be only the present invention several specific embodiments.Obviously, the present invention is not
It is limited to above example, acceptable there are many deformations.Those skilled in the art can be direct from present disclosure
All deformations for exporting or associating, are considered as protection scope of the present invention.
Claims (8)
1. extracting the technique of Sophoricoside from the Fructus Sophorae comprising following steps：
Crushing → high pressure → electric field treatment → shearing → enzyme reaction → microwave alcohol extracting → evaporation → drying → absorption → elution → steaming
Hair → drying → dissolving → crystallization.
2. extraction process according to claim 1, which is characterized in that the extraction process includes the following steps：
The Fructus Sophorae is taken, is crushed, 100-200 mesh sieve is crossed, obtains fructus sophorae powder, be subsequently placed in reactor, controlling pressure in reactor is
2-3MPa, pressurize 30-40s carry out impulse electric field processing；The water for adding 3-5 times of weight again, is sheared using high-speed shearing machine, so
Addition cellulase carries out enzyme reaction afterwards, then adds 70% ethyl alcohol of same volume, 60 DEG C is warming up to, using Microwave Extraction；It crosses
Extracting solution is collected in filter；Then into rotary evaporator, evaporation under reduced pressure removed ethyl alcohol, then vacuum freeze drying is obtained total
Flavones crude extract, then adsorbed with macroporous absorbent resin, with 70% ethanol elution, eluent is collected, rotation is re-introduced into and steams
It sends out in device, extractive of general flavone is made in evaporation under reduced pressure removed ethyl alcohol, vacuum freeze drying；Five times are added into extractive of general flavone
The ethyl acetate of weight, stirs evenly, and then filters, and collects insoluble matter, then 85% ethyl alcohol is added dropwise into insoluble matter, when being added dropwise
Heating, while being stirred with 100rpm, until insoluble matter is completely dissolved, it is subsequently placed in 30min under 0 DEG C of environment, is filtered, crystallization is collected
Object to get.
3. extraction process according to claim 2, which is characterized in that the field strength 10kv/cm of the impulse electric field, it is total to handle
Time is 200 μ s, and pulse width is 4 μ s, pulse frequency 400pps.
4. extraction process according to claim 2, which is characterized in that the shear time 3min of the high-speed shearing machine is cut
Cutting speed degree is 5000rpm.
5. extraction process according to claim 2, which is characterized in that the enzyme reaction condition is：According to 10,000-2 ten thousand U:
The ratio of 100g fructus sophorae powders adds cellulase, and control enzyme reaction temperature is 35 DEG C, reaction time 60-90min.
6. extraction process according to claim 2, which is characterized in that the condition of the Microwave Extraction is power 400-
600W, extraction time 30-50min.
7. Sophoricoside prepared by the extraction process according to claim 1-6.
8. purposes of the Sophoricoside described in claim 7 in anti-inflammatory.
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